Characterization of municipal solid waste incineration (MSWI) bottom ash by scanning electron microscopy and quantitative energy dispersive X-ray microanalysis (SEM/EDX)

Scanning electron microscopy (SEM) with energy-dispersive X-ray microanalysis (EDX) is frequently used for morphological and qualitative chemical characterization of different materials. The applicability of this method for phase identification, is, however, often underestimated. The application of SEM/EDX for the characterization of different phases in fresh and altered municipal-waste incinerator bottom-ash samples with high lateral resolution is presented. Polished thin sections were prepared from the samples, but fresh fracture surfaces were also used. The EDX analyses were performed by using the correction procedures of a conventional standardless ZAF correction, a peak-to-background ZAF correction, and a correction method for light-element analysis. Because of their highly reactive properties the bottom-ash SEM samples require a special method of preparation. The method facilitates nondestructive preparation of the sensitive bottom-ash alteration phases (e.g. cement phases, hydroxides, salts) and their microstructures. Received: 18 August 2000 / Revised: 8 November 2000 / Accepted: 12 November 2000     

Individual extraction constants of some univalent cations in the two-phase water–phenyltrifluoromethyl sulfone system

The preparation and characterization of three different phases of zirconium phosphate (ZrP) have been carried out using XRD, SEM, EDX, and FTIR spectroscopy. The phases exchange and sorption properties with three different radioisotope ²³⁴Th, ²³⁸U, and ¹³⁴Cs were investigated.     

Influence of different correction models on investigations of carbonaceous insulating films by electron beam X-ray microanalysis

Normally quantitative investigations of insulators by electron beam X-ray microanalysis are made possible by coating special samples with thin evaporated carbon films. This, however, will fail if the samples themselves contain carbon as polysilastyrene {[(CH₃)₂Si]_x (CH₃)C₆H₅Si}_n, which is used for the preparation of silicon carbide. Samples of polysilastyrene, together with reference layers (pure silicon) were investigated using different equipment (JEOL, CAMECA) and with varying correction procedures (ZAF, PAP). Compared with the results of reference measurements (elementary analysis, NMR) it appears that the PAP correction procedure is better suited for solving this problem than the classical ZAF correction procedure.     

X-ray and scanning electron microscopy archaeometric studies of pigments from the Aguada culture, Argentina

X-ray diffraction (XRD) and scanning electron microscopy (SEM) with energy-dispersive system (EDX) were used in order to obtain mineralogical and chemical composition of white and reddish pigments belonging to the Ambato style of “Aguada” culture, found in the archaeological site of Piedras Blancas (Catamarca, Argentina 500–1100 AD). These pigments are associated with different sectors, two of them being related to funerary context. Due the scarce amount of samples available, it was necessary to develop a new methodology for their study. X-ray diffraction spectra were collected using a low background Si sample holder, which allows the study of small sample amounts (a few milligrams). The mineral quantifications were carried out by applying the Rietveld method to the XRD spectra. The major difficulties arose for reddish pigments, since they contain iron-bearing phases, such as ferruginous clays, in which neither the concentration of Fe^{+ 2} relative to Fe^{+ 3} nor the location in the lattice (occupancy factor) is completely known. With the aim of performing quantitative elemental analysis from SEM-EDX spectra, a special sample holder for the small amounts of available samples was developed. Commercial standards were used in the quantification process and the characteristic intensities were corrected for matrix effects. Micrographs and EDX point spectra allowed the characterization of minor phases and particle analysis. The Rietveld method combined with the new procedure for EDX analysis has proven to be a suitable method for routine quantitative analysis of small amounts of archaeological pigments.     

Molecular and elemental characterisation of mineral particles by means of parallel micro-Raman spectrometry and Scanning Electron Microscopy/Energy Dispersive X-ray Analysis

The “fingerprinting” of a molecular structure obtained by micro-Raman spectroscopy (MRS) can be successfully complemented by means of X-ray spot analysis through the application of scanning electron microscopy equipped with an X-ray detector (SEM/EDX). The elemental composition revealed by SEM/EDX is essential for a correct interpretation of the collected Raman spectra. The results presented here illustrate how the two techniques can be combined to characterize geological samples, especially in the case of individual particles. The samples involved in the experiments were Zr- and Ti-bearing sand from South Africa (with major minerals such as zircon and rutile) and U mine tailings from Hungary (rich with feldspars, quartz and sulphate minerals). Mineral phases detected by MRS were identified according to their respective main Raman shifts, with a spatial resolution up to 1 μm, depending on the parameters set. Some unusual and sometimes inexplicable Raman activity was observed, which was ascribed to and rationalized by the presence of accompanying elements as detected with EDX. The relocation of a particle by means of the two instruments was facilitated with TEM grids. Although the limitations of the sequential use of SEM/EDX and MRS, such as different beam sizes, probing depth and surface topography, should be considered in their application to the analysis of individual geological particles, the two methods appeared to be complementary. Not only do they provide correlated chemical information about the sample, but also enable chemical characterization that would be otherwise incomplete when analyzed on a stand-alone basis.     

X-ray and scanning electron microscopy archaeometric studies of pigments from the Aguada culture,Argentina

X-ray diffraction (XRD) and scanning electron microscopy (SEM) with energy-dispersive system (EDX) were used in order to obtain mineralogical and chemical composition of white and reddish pigments belonging to the Ambato style of “Aguada” culture, found in the archaeological site of Piedras Blancas (Catamarca, Argentina 500–1100 AD). These pigments are associated with different sectors, two of them being related to funerary context. Due the scarce amount of samples available, it was necessary to develop a new methodology for their study. X-ray diffraction spectra were collected using a low background Si sample holder, which allows the study of small sample amounts (a few milligrams). The mineral quantifications were carried out by applying the Rietveld method to the XRD spectra. The major difficulties arose for reddish pigments, since they contain iron-bearing phases, such as ferruginous clays, in which neither the concentration of Fe^+ 2 relative to Fe^+ 3 nor the location in the lattice (occupancy factor) is completely known. With the aim of performing quantitative elemental analysis from SEM-EDX spectra, a special sample holder for the small amounts of available samples was developed. Commercial standards were used in the quantification process and the characteristic intensities were corrected for matrix effects. Micrographs and EDX point spectra allowed the characterization of minor phases and particle analysis. The Rietveld method combined with the new procedure for EDX analysis has proven to be a suitable method for routine quantitative analysis of small amounts of archaeological pigments.     

The adaptability of Cu/Zr oxides as oxygen carrier used for chemical looping air separation (CLAS)

Chemical looping air separation (CLAS), based on the chemical looping principle, is a novel and energy-efficient method to separate oxygen from air. The oxygen carriers used capture oxygen from air in an oxidation reactor and release oxygen in a reduction reactor. In this work, the adaptability of Cu/Zr oxygen carrier used for CLAS was investigated through thermodynamic analysis and experimental methods. X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to measure the phases and surface morphology of oxygen carriers before and after experiments. The results show that CuO has the capability of releasing oxygen when the temperature is higher than 725 °C in the nitrogen atmosphere, and the minimum oxygen reduction temperatures increase with the increasing of oxygen concentrations. The Cu/Zr oxygen carrier has high oxygen reduction and oxidation rates when temperature is higher than a certain values. For reduction, the value is about 860 °C. For oxidation, the value is about 500 °C. The reactivity of oxygen carrier increases significantly with the temperature increasing. On overall, reactivity of oxygen carrier has little difference under different particle sizes. The oxygen carrier exhibits a stable oxygen reduction and oxidation behavior during reduction–oxidation cycles. XRD patterns show that the main phases in reduced samples are Cu₂O and ZrO₂. The main phases in fresh and oxidized samples are CuO and ZrO₂. SEM images show that the fresh and reacted oxygen carriers are porous. The surface of reacted samples is smoother than fresh samples and no agglomeration has been found.     

Van Gogh’s Painting Grounds: Quantitative Determination of Bulking Agents (Extenders) Using SEM/EDX

A pre-concentration procedure using cloud point extraction is presented for the determination of uranium in natural water using molecular absorption spectrometry. The ligand used was 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol (Br-PADAP) and the micellar phase was obtained using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation. Interferences were eliminated using a masking solution containing trans-1,2-cyclohexanediaminetetraacetic acid (CDTA), sodium fluoride and sulphosalicylic acid. The optimization step was performed using a two-level factorial design and a Doehlert matrix, involving the factors pH, centrifugation time and buffer concentration. The method allows the determination of uranium in water samples with a detection limit of 0.15 μg L⁻¹, a quantification limit of 0.50 μg L⁻¹ and a precision expressed as relative standard deviation of 1.8 and 2.3% for uranium concentrations of 5 and 10 μg L⁻¹, respectively (n = 8). The accuracy was confirmed by analysis of two certified samples of natural water. This method was applied to the determination of uranium in superficial water samples collected at a uranium mine in Brazil. For five samples analyzed, the concentration of uranium varied between 1.1 and 18.1 μg L⁻¹. Tests of addition/recovery were performed for all these samples, and the results varying between 98 and 105% also proved that this procedure is not affected by the matrix and can be applied satisfactorily to the determination of uranium in water samples.     

Preparation and characterization of hybrid membranes for fuel cell applications: EPDM filled with organophilized silicas

This work reports on the preparation and characterization of hybrid membranes based on blends of ethylene‐propylene‐diene terpolymer (EPDM) and different organophilized silicas. The films obtained were crosslinked to improve mechanical stability, and heterogeneously sulfonated to convert them in proton conducting systems. The structural characterization consisted on the analysis of their thermal and mechanodynamical transitions by DSC and DMA, the verification of the introduction of sulfonic groups by infrared spectroscopy (ATR), and the obtaining of information about the silica location and distribution within the polymer by scanning electronic microscopy (SEM‐EDX). The electrical characterization was made using electrochemical impedance spectroscopy (EIS). Also, methanol crossover and water up‐take were determined, and the results were compared with those of Nafion^®117. Results show that sulfonation of the styrene rings has effectively occurred. Conductivity value is higher and methanol crossover is lower than in Nafion for all experimental samples. © 2009 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 47: 1203–1210, 2009     

Characterization of transition metal nitride formation in rapid thermal processing (RTP)

The potential of RTP for the preparation of transition metal nitrides by reaction of metal thin films in molecular nitrogen was investigated. The films and the nitridation process were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), energy dispersive x-ray analysis (EDX) in a scanning electron microscope (SEM) and secondary neutral mass spectrometry (SNMS). The chemical states of vanadium at the utmost surface, detected by XPS, are related to V₂O₅ before RTP and to vanadium nitride, oxide and oxynitride after RTP. The deposition of a 3 nm Si top layer prevents V from oxidation and its selective removal before RTP enhances the proportion of nitride determined by XPS after RTP. From comparative experiments in a conventional tube furnace the advantages of RTP became obvious. With short process times of the RTP technique the integral amount of residual oxygen is kept low and oxide formation is largely avoided. The nitrogen content and the different polycrystalline phases formed by varying process time and temperature provide information about reactivity and the nitridation process. The nitrogen to vanadium ratio was determined by EDX and SNMS, revealing that the N content reaches saturation after only 5 seconds at 1100?°C.     

Possibility of scanning electron microscope observation and energy dispersive X-ray analysis in microscale region of insulating samples using diluted ionic liquid

The possibility of scanning electron microscope (SEM) observation and energy dispersive X-ray (EDX) spectrometry analysis in microscale regions of insulating samples using diluted ionic liquid was investigated. It is possible to obtain clear secondary electron images of insulating samples such as a rock and mineral at 5,000 times magnification by dropping 10 μL of 1 wt% of 1-ethyl-3-methylimidazolium acetate (EMI-CH?COO) diluted with ethanol onto the samples. We also obtained EDX spectra of the samples in microscale regions (~5 μm2) without overlapping EDX spectra of other minerals with different composition. It might be possible to perform quantitative analysis of the samples if a method that does not need standard samples is applied or an X-ray detector sensitive for light elements was attached. The method of dropping 1 wt% EMI-CH?COO diluted with ethanol onto insulating samples is useful for SEM observation, EDX analysis in microscale regions, and the preservation of scarce rock and mineral samples because ionic liquid can be easily removed with acetone.     

Two-layered Au@Ag Bimetallic Nanocomposites-poly (L-Met) Platform for Highly Sensitive Chlorpheniramine Maleate Detection

The two-layered bimetallic Au@Ag and poly(L-methionine) (Au@Ag/p-L-met) sensor was newly developed for the electrochemical determination of chlorpheniramine maleate (CPM). After electropolymerization of L-met, bimetallic surfaces were prepared by electrodeposition of Au@Ag nanoparticles on the p-L-met/PGE. The surface characterization was carried out by scanning electron microscopy (SEM), Energy Dispersive X-ray spectroscopy (EDX), Cyclic Voltammetry (CV) and Electrochemical impedance spectroscopy (EIS). The sensor shows good electrocatalytic activity, high sensitivity, wide linear range (0.87–600.0 μM) and a low detection limit (0.26 μM) by using Differential pulse voltammetry (DPV). The sensor was used to determine CPM in pharmaceutical samples with satisfactory results.     

用扫描电镜和能谱仪进行金矿鉴定的研究

运用扫描电子显微镜（ＳＥＭ）及Ｘ射线能谱仪（ＥＤＸ）进行金矿鉴定的实验研究，结果表明，本法比较直观、简便，可以确定金的存在形式及生成环境，并鉴定金矿物的种类     

Preparation and electrochemical performances of silver (alloy) nanoparticles decorated on reduced graphene oxide,using self-polymerization of dopamine in an acidic environment

Self-polymerization of dopamine, in either an alkaline or an acidic environment, to form polydopamine is a material-independent surface coating technique, influencing almost all areas of material science and engineering. We demonstrated a simple, two-step method to prepare in-situ silver or silver-copper alloy nanoparticles on the surface of reduced graphene oxides, using polydopamine formed in an acidic medium. The acidic medium was created by a nonthermal micro-hollow cathode discharge device and the device was operated at atmospheric pressure, using air as the working gas. The nanocomposites were characterized with SEM, EDX, ICP-OES, and FT-IR; the electrochemical catalytic activity was tested using rotating disk electrode. The characterization methods confirmed the formation of the nanocomposites, which contain polydopamine, reduced graphene oxides, and metal nanoparticles or nanoalloy. We hypothesized that by alloying silver and copper on the surface of reduced graphene oxides, the oxygen reduction reaction (ORR) catalytic activity of the nanocomposites will be enhanced through both alloying and substrate effects. The size range of the nanoparticles is between 10 nm and 15 nm. We find that both the silver and alloy samples catalyze the ORR via a four-electron mechanism. The alloy nanocomposites showed better performance indicator parameters than the silver one, in both mass activity and kinetic current density. This preparation method has paved a new way of synthesizing an ORR catalyst in an environmentally friendly manner.     

Synthesis and Properties of Zeolites from Autoclaved Aerated Concrete (AAC) Waste

Syntheses routes for the conversion of autoclaved aerated concrete (AAC) waste into aluminosilicate zeolites like LTA and related phases were developed. The procedures always started with leaching steps of the pure AAC waste by combinations of strong alkaline (NaOH) and mild acid (citric acid) treatments, before the real crystallization process was performed separately under addition of sodium aluminate. All products were characterized by X‐ray powder diffraction (XRD), scanning electron microscopy (SEM) combined with energy dispersive X‐ray analysis (EDX‐analysis) and Fourier‐transform infrared spectroscopy (FTIR). Zeolites LTA and related phases basic sodalite (SOD), hydrosodalite (SOD), cancrinite (CAN) and an intermediate phase between SOD and CAN were observed. Depending on the preparation route tailor made synthesis of pure phase zeolite LTA with crystal sizes up to 5 μm was worked out. In addition to syntheses procedures important properties of the zeolites were discussed with respect to the treatment procedure of AAC. It is shown, that the special synthesis pathway is not only responsible for the product composition and formation of a certain structure type but also exhibits a strong influence on the crystallinity, crystal size, and morphology. The water sorption capacity and the hydrothermal stability of the products were selected for those further investigations. Whereas adequate water sorption capacity up to 272 mg · g^–1 were measured for zeolites LTA obtained from two different reaction routes, limited hydrothermal stabilities were revealed for other products. Under the conditions of strong hydrothermal treatment at a temperature of 473 K for 72 h, a more or less extended phase transformation into ANA‐Type zeolites occurred. This process was least extensive for pure phase zeolite LTA obtained from the alkaline solution of AAC leaching.     

Physicochemical characterization of chitin from the Mediterranean flour moth,Ephestia kuehniella Zeller (Lepidoptera: Pyralidae)

Moth chitin was extracted from adult of the Mediterranean flour moth by alkali-acid treatment and its characteristics were investigated and compared with shrimp chitin because the specific applications of chitin is directly associated with its physicochemical properties. The results revealed that the moth contained significant amounts of chitin but lower amounts of minerals. Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), scanning electron microscopy (SEM) and energy dispersive x-ray diffraction (EDX) were used to investigate physicochemical characteristics of chitin samples. FT-IR spectra revealed that the moth chitin had α-chitin form (anti-parallel chains) with respect to the different orientations of its microfibrils. The degree of acetylation of chitin from moth and shrimp calculated using the FT-IR stretching bands were 70.82% and 71.42%, respectively. The SEM observation exhibited the presence of fibrillar material and porous structures in surface of the chitin samples. EDX analysis revealed that the main elements present in the moth chitin (beyond C, O and N) were Br (10.5%) and Si (9.7%). Our study of enzymatic activity toward colloidal chitin as substrate showed that the extracted chitin from E. kuehniella had high chemical purity as well as commercial chitin.     

High-performance liquid chromatographic stationary phases based on poly(dimethylsiloxane) immobilized on silica

This work describes the preparation and characterization of six stationary phases for high-performance liquid chromatography (HPLC) obtained by deposition of poly(dimethylsiloxane) (PDMS) in HPLC silica particles, followed by immobilization using different processes (thermal treatments, thermal treatment + microwave irradiation, self-immobilization + gamma irradiation and self-immobilization + microwave irradiation). The chromatographic parameters of all the phases were evaluated with a mixture of test compounds having varied natures (acid, basic and neutral). The stability of one of these phases was evaluated in both a neutral mobile phase and a higher pH mobile phase used at an elevated temperature, with promising results.     

Determination of colloidally-associated polycyclic aromatic hydrocarbons (PAHs) in fresh water using C18 solid phase extraction disks

A new application of reversed-phase octadecyl (C₁₈) solid phase extraction disks has been developed to separate the colloidally-associated polycyclic aromatic hydrocarbons (PAHs) from those that were truly dissolved in the samples of fresh water. A correction for the retention of small amounts of colloidal material on the C₁₈ disks was required, which would have otherwise lead to minor underestimates in the degree of partitioning between the two phases. Using the humic substance Aldrich Humic Acid (AHA) as a model colloid and the 16 PAHs on the US Enrivonmental Protection Agency priority pollutant list, the partitioning coefficients of the PAHs between the colloidal and truly dissolved phases were shown to be proportional to the hydrophobicity of the PAHs, as measured by their octanol water partition coefficients (K_ow). The values for the partition coefficients obtained (cK_doc′) were similar to those previously reported in the literature using alternative methods, confirming that the technique was producing acceptable results. The technique allows the in situ partitioning of PAHs between the truly dissolved and colloidal phases in fresh water bodies to be determined. It will provide an invaluable cross-check of the laboratory-based methods which often require substantial manipulation of the sample and potentially alter the partitioning between the phases.     

Electrocatalytic Investigations of Cu(II) and Fe(III) Complexes of Salophen Derivative Schiff Bases on the Pencil Graphite Electrode

This present study describes a pencil graphite electrode surface covered with Cu(II) and Fe(III) complexes based on Salophen derivative Schiff bases in acetonitrile solution containing LiClO₄ as a supporting electrolyte. Cyclic voltammetry method was used for the surface modification procedure with 25 cycle at a sweep rate of 50 mV s^?1. Some characterization methods were used to identify of the prepared modified surfaces including cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), Ultraviolet‐visible Spectroscopy (UV‐Vis), and Scanning Electron Microscopy/Energy Dispersive X‐ray Spectroscopy (SEM/SEM‐EDX). The catalytic activity of these modified surfaces on the electrochemical oxidation of catechol (CC) was investigated and they compared with each other. The results demonstrated that these modified electrodes showed perfect electrocatalytic activity on the catechol determination, however the modified electrode prepared with the Cu(II) complex has higher catalytic activity than this prepared with the Fe(III) complex thanks to its the lower detection limit.     

Synthesis of colloidal nanoscaled copper-indium-gallium-selenide (CIGS) particles for photovoltaic applications

In this work, Cu(In,Ga)Se(2) (CIGS) nanoparticles were synthesized using a wet chemical method. The method is based on a non-vacuum thermal process that does not use selenization. The effects of temperature, source materials, and growth conditions on the phase and particle size were investigated. X-ray diffraction results confirm the formation of a tetragonal CIGS structure as the main phase with the purity more than 99% obtained by energy-dispersive X-ray spectroscopy (EDX). The morphology and size of the samples were investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Using these methods, 20-80nm particles were obtained. Through measurements of the absorption spectra of CIGS nanoparticles, the band gap of the synthesized material was determined to be about 1.44eV, which corresponds to an acceptable wavelength region for absorber layers in solar cells.